CN105314982B - The preparation method and application of ternary multi-ferroic material, the material - Google Patents
The preparation method and application of ternary multi-ferroic material, the material Download PDFInfo
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Abstract
The present invention relates to Material Field, in particular to the preparation method and application of a kind of ternary multi-ferroic material, the material.The chemical composition of the material is：xBiFeO3‑(1‑x‑y)Pb(Fe1/ 2NbO1/2)O3‑yPbTiO3；Wherein, 0<x≤0.5；0.1≤y≤0.3.The preparation method comprises the following steps：(1) initial feed is weighed according to the stoichiometric proportion of molecular formula；(2) the initial feed mixed grinding that will be weighed up, then tabletting, and synthesize, pre-synthesis sample is made；(3) pre-synthesis sample is continued to grind, adds PVA afterwards as binding agent, tabletting back glue；(4) will be sintered in the tabletting high temperature after dumping.Application of the ternary multi-ferroic material in sensor or driver.The ternary multi-ferroic material that the embodiment of the present invention is provided has excellent stability, electric property and magnetic property, can be applied in sensor or driver.
Description
Technical field
The present invention relates to Material Field, in particular to a kind of ternary multi-ferroic material, the material preparation method and
Using.
Background technology
Early in P Curie in 1894 just using the theoretical prediction nature of symmetry in magnetoelectric effect be present.Nineteen sixty section
Scholars are found that monocrystalline Cr2O3Magnetoelectric effect within the temperature range of 80K to 330K be present, thus triggered searching magnetoelectricity to imitate
The upsurge answered, and Ca-Ti ore type magnetic ferroelectric material is being mixed in succession, it is found that in antiferromagnet and ferrimagnetic material extremely weak
Magnetoelectric effect.1970, Aizu had a series of similitude to be attributed to one according to ferroelectricity, ferromagnetic, three kinds of properties of iron bullet
Class, it is proposed that the concept of ferroic material (ferroics).The Schmid of Switzerland in 1994 clearly proposes multi-ferroic material
(multi-ferroic) concept, the single-phase compounds with two or more primary ferroic feature are referred to.In Fragrance Hill section
In association's the 306th academic discussion of view, the modification of bismuth ferrite-titanate lead solid solution system and more iron are described to expert system
Property.It is bright that result of study shows that the cation-modified bismuth ferrite such as lanthanum, gallium-lead titanates solution ceramic system various aspects of performance has
It is aobvious to improve.At the quasi- homotype phase boundary of the system, the performance such as its structure, electricity, magnetics can be designed by component into
Row is cut out, and polarization and the magnetizability significantly improved is shown compared with ferrous acid bismuth single crystal.In application aspect, such material can use
In electronic devices such as novel sensor, drivers.However, the report of the ternary system related to bismuth ferrite-lead titanates but lacks it
It is again few.
The content of the invention
In a first aspect, the invention provides a kind of Stability Analysis of Structures, electric property and the ternary multiferroic material having excellent magnetic characteristics
Material；Second aspect, the invention provides a kind of preparation method of ternary multi-ferroic material；The third aspect, the invention provides one
Application of the kind ternary multi-ferroic material in sensor or driver.
According to the embodiment of the present disclosure in a first aspect, the ternary multi-ferroic material provided, the chemical composition of the material are：
xBiFeO3-(1-x-y)Pb(Fe1/2NbO1/2)O3-yPbTiO3；
Wherein, 0<x≤0.5；0.1≤y≤0.3.
In above-mentioned ternary multi-ferroic material, 0.25≤x≤0.5；0.1≤y≤0.2.
In above-mentioned ternary multi-ferroic material, x=0.25；0.1≤y≤0.16.
According to the second aspect of the embodiment of the present disclosure, the preparation method of the ternary multi-ferroic material provided, including it is following
Step：
(1) by initial feed according to xBiFeO3-(1-x-y)Pb(Fe1/2Nb1/2)O3-yPbTiO3The stoichiometry of molecular formula
Than being weighed；
(2) the initial feed mixed grinding 1-3h that will be weighed up, then in 3-5MPa lower sheetings, and is closed at 700-900 DEG C
Into 3-5h, pre-synthesis sample is made；
(3) pre-synthesis sample is continued to grind 1-3h, adds PVA that mass concentration is 5% afterwards as binding agent,
180-220MPa lower sheetings, then in 400-600 DEG C of dumping 1-3h hour；Wherein, it is corresponding to weigh 0.01mol ternary multiferroic materials
Pre-synthesis sample made of initial feed needed for material, the PVA amounts added are 4-6 drops；
(4) tabletting after dumping is put into sintering 2-4 hours in 1000 DEG C of -1050 DEG C of high temperature.
In the preparation method of above-mentioned ternary multi-ferroic material, the initial feed in the step (1) includes PbO, Bi2O3,
Fe2O3, Nb2O5, and TiO2。
In the preparation method of above-mentioned ternary multi-ferroic material, in the step (2), the initial feed weighed up is added into nothing
Water-ethanol mixed grinding 2h, then in 4MPa lower sheetings, and 4h is synthesized at 800 DEG C.
In the preparation method of above-mentioned ternary multi-ferroic material, in the step (3), pre-synthesis sample is added into anhydrous second
Alcohol continues to grind 2h, adds PVA that mass concentration is 5% afterwards as binding agent, in 200MPa lower sheetings, then 500
DEG C dumping 2h hours.
In the preparation method of above-mentioned ternary multi-ferroic material, in the step (4), the tabletting after dumping is put into 1000
Sintered 3 hours in DEG C -1050 DEG C of high temperature.
In the preparation method of above-mentioned ternary multi-ferroic material, in the step (2) and step (3), before grinding first
Add absolute ethyl alcohol；Wherein, the corresponding initial feed weighed needed for 0.01mol ternary multi-ferroic materials, the anhydrous second added
Alcohol amount is 10-20ml.
According to the third aspect of the embodiment of the present disclosure, the ternary multi-ferroic material provided is in sensor or driver
Using.
The technical scheme provided by this disclosed embodiment can include the following benefits：
Ternary multi-ferroic material prepared by the preparation method that the embodiment of the present invention is provided has excellent stability, electrical property
Energy and magnetic property, it can be applied in sensor or driver.
It should be appreciated that the general description and following detailed description of the above are only exemplary, this can not be limited
It is open.
Brief description of the drawings
The XRD diffraction patterns for the ternary multi-ferroic material that Fig. 1 is drawn by experimental example one of the present invention for preparation example three to six
Spectrum；
The dielectric temperature for the ternary multi-ferroic material that Fig. 2 is drawn by experimental example two of the present invention for preparation example three to six is composed；
The ferroelectric hysteresis loop for the ternary multi-ferroic material that Fig. 3 is drawn by experimental example two of the present invention for preparation example three to six；
The hysteresis curve for the ternary multi-ferroic material that Fig. 4 is drawn by experimental example two of the present invention for preparation example three to six；
The M-T curves for the ternary multi-ferroic material that Fig. 5-8 is drawn by experimental example two of the present invention for preparation example three to six.
Accompanying drawing herein is merged in specification and forms the part of this specification, shows the implementation for meeting the present invention
Example, and for explaining principle of the invention together with specification.
Embodiment
The present invention is described in further detail below by specific examples of the implementation and with reference to accompanying drawing.
Preparation example one
Preparation chemical composition is xBiFeO3-(1-x-y)Pb(Fe1/2NbO1/2)O3-yPbTiO3Ternary multi-ferroic material；
Wherein, x=0.1；Y=0.1.
The ternary multi-ferroic material preparation process is as follows：(1) by initial feed PbO, Bi2O3, Fe2O3, Nb2O5, and TiO2
According to xBiFeO3-(1-x-y)Pb(Fe1/2Nb1/2)O3-yPbTiO3The stoichiometric proportion of molecular formula is weighed, and the amount of weighing is
The weight of initial feed corresponding to the 0.01mol ternary multi-ferroic materials；(2) the initial feed mixed grinding 3h that will be weighed up,
Then in 5MPa lower sheetings, and 3h is synthesized at 900 DEG C, pre-synthesis sample is made；(3) pre-synthesis sample is continued to grind 3h,
Add afterwards 6 drop mass concentrations be 5% PVA as binding agent, it is then small in 400 DEG C of dumping 3h in 220MPa lower sheetings
When；(4) tabletting after dumping is put into 1000 DEG C of high temperature and sintered 4 hours, obtain the ternary multi-ferroic material.
Preparation example two
Preparation chemical composition is xBiFeO3-(1-x-y)Pb(Fe1/2NbO1/2)O3-yPbTiO3Ternary multi-ferroic material；
Wherein, x=0.5；Y=0.2.
The ternary multi-ferroic material preparation process is as follows：(1) by initial feed PbO, Bi2O3, Fe2O3, Nb2O5, and TiO2
According to xBiFeO3-(1-x-y)Pb(Fe1/2Nb1/2)O3-yPbTiO3The stoichiometric proportion of molecular formula, the amount of weighing should for 0.01mol
The weight of initial feed corresponding to ternary multi-ferroic material；(2) the initial feed mixed grinding 1h that will be weighed up, then in 3MPa
Lower sheeting, and 5h is synthesized at 700 DEG C, pre-synthesis sample is made；(3) pre-synthesis sample is continued to grind 1h, adds 4 afterwards
PVA that mass concentration is 5% is dripped as binding agent, in 180MPa lower sheetings, then in 600 DEG C of dumping 1h hours；(4) by dumping
Tabletting afterwards is put into 1050 DEG C of high temperature and sintered 2 hours, obtains the ternary multi-ferroic material.
Preparation example three
Preparation chemical composition is xBiFeO3-(1-x-y)Pb(Fe1/2NbO1/2)O3-yPbTiO3Ternary multi-ferroic material；
Wherein, x=0.25；Y=0.1.
The ternary multi-ferroic material preparation process is as follows：(1) by initial feed PbO, Bi2O3, Fe2O3, Nb2O5, and TiO2
According to xBiFeO3-(1-x-y)Pb(Fe1/2Nb1/2)O3-yPbTiO3The stoichiometric proportion of molecular formula is weighed, and the amount of weighing is
The weight of initial feed corresponding to the 0.01mol ternary multi-ferroic materials；(2) it is the initial feed weighed up addition 10ml is anhydrous
Ethanol and mixed grinding 2h, then in 4MPa lower sheetings, and synthesize 4h at 800 DEG C, pre-synthesis sample are made；(3) will close in advance
10ml absolute ethyl alcohols are added into sample and continue to grind 2h, add PVA that 5 drop mass concentrations are 5% afterwards as binding agent,
In 200MPa lower sheetings, then in 500 DEG C of dumping 2h hours；(4) that the tabletting after dumping is put into 1000 DEG C of high temperature into sintering 3 is small
When, obtain the ternary multi-ferroic material.
Preparation example four
Preparation chemical composition is xBiFeO3-(1-x-y)Pb(Fe1/2NbO1/2)O3-yPbTiO3Ternary multi-ferroic material；
Wherein, x=0.25；Y=0.12.
The ternary multi-ferroic material preparation process is as follows：(1) by initial feed PbO, Bi2O3, Fe2O3, Nb2O5, and TiO2
According to xBiFeO3-(1-x-y)Pb(Fe1/2Nb1/2)O3-yPbTiO3The stoichiometric proportion of molecular formula is weighed, and the amount of weighing is
The weight of initial feed corresponding to the 0.01mol ternary multi-ferroic materials；(2) it is the initial feed weighed up addition 20ml is anhydrous
Ethanol and mixed grinding 2h, then in 4MPa lower sheetings, and synthesize 4h at 800 DEG C, pre-synthesis sample are made；(3) will close in advance
20ml absolute ethyl alcohols are added into sample and continue to grind 2h, add PVA that 5 drop mass concentrations are 5% afterwards as binding agent,
In 200MPa lower sheetings, then in 500 DEG C of dumping 2h hours；(4) that the tabletting after dumping is put into 1050 DEG C of high temperature into sintering 3 is small
When, obtain the ternary multi-ferroic material.
Preparation example five
Preparation chemical composition is xBiFeO3-(1-x-y)Pb(Fe1/2NbO1/2)O3-yPbTiO3Ternary multi-ferroic material；
Wherein, x=0.25；Y=0.14.
The ternary multi-ferroic material preparation process is as follows：(1) by initial feed PbO, Bi2O3, Fe2O3, Nb2O5, and TiO2
According to xBiFeO3-(1-x-y)Pb(Fe1/2Nb1/2)O3-yPbTiO3The stoichiometric proportion of molecular formula is weighed, and the amount of weighing is
The weight of initial feed corresponding to the 0.01mol ternary multi-ferroic materials；(2) the initial feed 20ml weighed up is added anhydrous
Ethanol and mixed grinding 2h, then in 4MPa lower sheetings, and synthesize 4h at 800 DEG C, pre-synthesis sample are made；(3) will close in advance
20ml absolute ethyl alcohols are added into sample and continue to grind 2h, add PVA that 5 drop mass concentrations are 5% afterwards as binding agent,
In 200MPa lower sheetings, then in 500 DEG C of dumping 2h hours；(4) that the tabletting after dumping is put into 1000 DEG C of high temperature into sintering 3 is small
When, obtain the ternary multi-ferroic material.
Preparation example six
Preparation chemical composition is xBiFeO3-(1-x-y)Pb(Fe1/2NbO1/2)O3-yPbTiO3Ternary multi-ferroic material；
Wherein, x=0.25；Y=0.16.
The ternary multi-ferroic material preparation process is as follows：(1) by initial feed PbO, Bi2O3, Fe2O3, Nb2O5, and TiO2
According to xBiFeO3-(1-x-y)Pb(Fe1/2Nb1/2)O3-yPbTiO3The stoichiometric proportion of molecular formula is weighed, and the amount of weighing is
The weight of initial feed corresponding to the 0.01mol ternary multi-ferroic materials；(2) it is the initial feed weighed up addition 10ml is anhydrous
Ethanol and mixed grinding 2h, then in 4MPa lower sheetings, and synthesize 4h at 800 DEG C, pre-synthesis sample are made；(3) will close in advance
10ml absolute ethyl alcohols are added into sample and continue to grind 2h, add PVA that 5 drop mass concentrations are 5% afterwards as binding agent,
In 200MPa lower sheetings, then in 500 DEG C of dumping 2h hours；(4) that the tabletting after dumping is put into 1050 DEG C of high temperature into sintering 3 is small
When, obtain the ternary multi-ferroic material.
Below using the gained ternary multi-ferroic material of preparation example one to six as experimental subjects, pass through three prepared by experimental analysis
The property and performance of first multi-ferroic material, it is specific as follows：
Experimental example one
The structure determination of ceramics：
Using X-ray powder diffraction, it is determined that the structure of ceramics.Instrument is Japanese RIGAKU-DMAX2500 powder
Diffractometer (Cu targets, λ=0.154056nm, graphite monochromator), specific test condition is at room temperature, measurement angle scope is 10-
80 °, the step-length used is 0.02 ° (2θ), time 2s/ steps.Obtained powder diffraction result is as shown in Figure 1.
Experimental example two
Electric property and the magnetic property measurement of ceramics
A) elargol is coated from ceramics section wear down, polishing, two sides, the measurement for electric property.
B) measurement of dielectricity：Instrument be Alpha's dielectric/impedance Analytical high resolution instrument (Novolcontrol,
German), 30~500 DEG C of temperature-measuring range, 1~10kHz of frequency range, small-signal test voltage 1Vrms.
C) ferroelectric measurement：Instrument is TF2000 standard ferroelectricity measuring systems, and temperature conditionss are room temperature, added frequency
Rate is 4Hz.
D) test of magnetic property：Hysteresis curve instrument is PPMS-9T, tests and is carried out under 5K, instrument used in M-T curves
Device is MPMS-XL, and temperature range is from 0K-300K.
The present invention is carried out based on new multi-ferroic material is found.BiFeO3-Pb(Fe1/2Nb1/2)O3-PbTiO3(letter
Claim BF-PFN-PT) as having ferroelectricity and anti-ferromagnetic multi-ferroic material, there is good researching value and practical valency
Value.It is ceramic building-up process first, by experimental exploring repeatedly, explores optimal synthesis temperature, generated time, sintering temperature
Degree and sintering time, finally give the optimal ceramics sample of performance, structure are determined with X-ray powder diffraction, then, to its electricity
Learn performance and magnetic performance carries out test analysis.
Understood through XRD powder test analysis, preparation example one is pure three with the ternary multi-ferroic material in preparation example two
Square Perovskite Phase, magnetometric analysis understand that the material is anti-ferromagnetism.
The residual polarization of preparation example one and coercive field are respectively 19.8 μ C/cm2Show this with the test of 12.42kV/cm. piezoelectricity
The piezoelectric modulus of the material of component is 223pC/N.
The electrical testing of preparation example two can also obtain more perfect ferroelectric hysteresis loop, and residual polarization is 14.57 μ C/cm2, coercive
Field is 22.24kV/cm.Piezoelectricity test shows that the piezoelectric modulus of the material of the component is 50pC/N.
The specific measurement result of preparation example three to six is as shown in Fig. 2-Fig. 8.Its Curie temperature is from 146 DEG C~309 DEG C；Rectify
Stupid field is effectively reduced, from 3.72kV/cm~22.24kV/cm；Piezoelectric modulus reaches 351pC/N.
Because it possesses above-mentioned premium properties, therefore can be applied in sensor or driver, it is existing to substitute
Ferroic material.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (8)
1. a kind of ternary multi-ferroic material, it is characterised in that the chemical composition of the material is：xBiFeO3-(1-x-y)Pb(Fe1/ 2NbO1/2)O3-yPbTiO3；
Wherein, x=0.25；0.1≤y≤0.16；
The Curie temperature of the ternary multi-ferroic material is 146 DEG C~309 DEG C, and coercive field is 3.72kV/cm~22.24kV/cm.
2. the preparation method of the ternary multi-ferroic material described in claim 1, it is characterised in that comprise the following steps：
(1) by initial feed according to xBiFeO3-(1-x-y)Pb(Fe1/2Nb1/2)O3-yPbTiO3The stoichiometric proportion of molecular formula is entered
Row is weighed；
(2) the initial feed mixed grinding 1-3h that will be weighed up, then in 3-5MPa lower sheetings, and synthesizes 3- at 700-900 DEG C
5h, pre-synthesis sample is made；
(3) by pre-synthesis sample continue grind 1-3h, add afterwards mass concentration be 5% PVA as binding agent, in 180-
220MPa lower sheetings, then in 400-600 DEG C of dumping 1-3h；Wherein, it is corresponding to weigh needed for 0.01mol ternary multi-ferroic materials
Pre-synthesis sample made of initial feed, the PVA amounts added are 4-6 drops；
(4) tabletting after dumping is put into sintering 2-4 hours in 1000 DEG C of -1050 DEG C of high temperature.
3. the preparation method of ternary multi-ferroic material according to claim 2, it is characterised in that in the step (1)
Initial feed includes PbO, Bi2O3, Fe2O3, Nb2O5, and TiO2。
4. the preparation method of ternary multi-ferroic material according to claim 2, it is characterised in that, will in the step (2)
The initial feed weighed up adds absolute ethyl alcohol mixed grinding 2h, then in 4MPa lower sheetings, and synthesizes 4h at 800 DEG C.
5. the preparation method of ternary multi-ferroic material according to claim 2, it is characterised in that, will in the step (3)
Pre-synthesis sample, which adds absolute ethyl alcohol, to be continued to grind 2h, adds PVA that mass concentration is 5% afterwards as binding agent,
200MPa lower sheetings, then in 500 DEG C of dumping 2h.
6. the preparation method of ternary multi-ferroic material according to claim 2, it is characterised in that, will in the step (4)
Tabletting after dumping is put into 1000 DEG C of -1050 DEG C of high temperature and sintered 3 hours.
7. the preparation method of the ternary multi-ferroic material according to any one of claim 2 to 6, it is characterised in that the step
Suddenly in (2) and step (3), absolute ethyl alcohol is first added before grinding；Wherein, it is corresponding to weigh 0.01mol ternary multi-ferroic materials
Required initial feed, the absolute ethyl alcohol amount added are 10-20ml.
8. application of the ternary multi-ferroic material in sensor or driver described in claim 1.
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